CN109768269A - The porous carbon coating tin dioxide composite material of nitrogen sulphur codope, preparation method and application - Google Patents
The porous carbon coating tin dioxide composite material of nitrogen sulphur codope, preparation method and application Download PDFInfo
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Abstract
The invention discloses porous carbon coating tin dioxide composite materials of a kind of nitrogen sulphur codope and preparation method thereof, comprising the following steps: phenolic resin is added in organic solvent, stirring and dissolving is subsequently added into stannic oxide particle, obtains reaction solution；2,5- dimercapto-1,3,4-thiadiazole is added in organic solvent, mixed dissolution, is subsequently added into reaction solution, cetyl trimethylammonium bromide is added, ammonium persulfate-methanol-water solution is added, for 24 hours, revolving obtains reactant for stirring；S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, calcines 5h at 700~900 DEG C under protective gas atmosphere then to get composite material is arrived.The present invention also provides application of the composite material on cathode of lithium battery.Composite material of the present invention avoids active material that dusting occurs in charge and discharge process by the doping of the buffering and N, S element of soft charcoal layer, significantly improves circulation ability and rate capacity.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of porous carbon coating stannic oxide of nitrogen sulphur codope is multiple
Condensation material and preparation method thereof.
Background technique
Growing energy demand needs better energy storage device, and lithium ion battery is due to its lightweight, and energy is close
Degree is high, environmental-friendly, long service life and be concerned.However currently commercially graphite material is low due to its theoretical capacity
(372mAhg-1) limitation lithium ion battery application.So we are badly in need of finding or create, a kind of energy density is high, cyclicity
The good material of energy.And granules of stannic oxide has very unique property, such as at low cost, theoretical capacity height (790mAhg-1), environmental protection
It is nontoxic.However the electric conductivity of stannic oxide is poor causes its high rate performance poor and Li/Li+Discharge potential it is lower, limitation
Application of the stannic oxide in electrochemical field.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of porous carbon coating titanium dioxides of nitrogen sulphur codope
Tin composite material, preparation method and application.
The first purpose of the invention is to provide a kind of systems of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope
Preparation Method, comprising the following steps:
S1, phenolic resin is added in organic solvent, stirring and dissolving is subsequently added into stannic oxide particle, at 40 DEG C
4h is reacted, reaction solution is obtained, wherein the molar ratio of phenolic resin and stannic oxide particle is 2.5~4:1；
S2, ammonium persulfate is added in methanol-water solution, dissolves, obtains ammonium persulfate-methanol-water solution；
S3,2,5- dimercapto-1,3,4-thiadiazole is added in organic solvent, mixed dissolution, then in stirring
Reaction solution obtained in lower addition S1 is added cetyl trimethylammonium bromide, continues to stir, and mistake obtained in S2 is then added
Ammonium sulfate-methanol-water solution, for 24 hours, revolving obtains reactant for stirring；Wherein, in stannic oxide particle used in S1 and S2
The ammonium persulfate that uses and with 2,5- dimercapto -1,3,4- thiadiazoles, cetyl trimethylammonium bromide used in S3
Molar ratio is 3~10:150~344:100:14；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, then in 700~900 under protective gas atmosphere
Calcine 5h at DEG C, cooled to room temperature is to get arriving the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
Preferably, in step S1, the ratio of phenolic resin and organic solvent is 0.3~0.5g:50ml.
Preferably, in step S2, the ratio of the ammonium persulfate and methanol-water solution is 6.85~7.85g:50ml.
Preferably, in step S2, the volume ratio of methanol and water is 1:1 in methanol-water solution.
Preferably, in step S3, the ratio of 2,5- dimercapto-1,3,4-thiadiazoles and organic solvent is 1.5~0.3g:
50ml。
Preferably, in step S1 and S3, the organic solvent is one of acetone, dehydrated alcohol.
Preferably, in step S4, the protective gas is argon gas.
Preferably, in step S4, the heating rate of the calcination process is 3 DEG C/min.
A second object of the present invention is to provide a kind of nitrogen sulphur codope porous carbon packets that above-mentioned preparation method is prepared
Cover tin dioxide composite material.
Third object of the present invention is to provide a kind of above-mentioned porous carbon coating tin dioxide composite materials of nitrogen sulphur codope
Application on cathode of lithium battery.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention is with phenolic resin and 2,5- dimercapto-1,3,4-thiadiazole (DMcT) respectively as carbon source and sulphur,
Nitrogen source is coated to synthetic nitrogen sulphur codope tin dioxide carbon nano-composite material on stannic oxide, hence it is evident that change electron density,
Lead to the strong interaction between Li-N and S-S, and the porous structure of composite material surface that synthesizes of the present invention is remarkably reinforced pair
The chemisorption of lithium ion；
(2) carbon-coating of the N-S doping in the present invention generates more defects and more activated centres, is conducive to storage more
More Li+Ion, and the doping of the buffering of soft charcoal layer and N, S element avoids active material that dusting occurs in charge and discharge process,
Thus, significantly improve the electrochemical cycleability and rate capacity of composite material；
(3) preparation method provided by the invention is at low cost, toxicity is low, easy to operate, mild condition, time-consuming is short, mechanism is clear
Chu has huge application prospect in terms of cathode of lithium battery.
Detailed description of the invention
Fig. 1 is the specific surface of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope prepared by the embodiment of the present invention 1
Long-pending and graph of pore diameter distribution；
Fig. 2 is the porous carbon coating tin dioxide composite material of nitrogen sulphur codope, comparative example 1 prepared by the embodiment of the present invention 1
750 chemical property curve graphs are recycled under 100mA/g current density with the material of 2 preparations；
Fig. 3 is the porous carbon coating tin dioxide composite material of nitrogen sulphur codope and comparative example 1 prepared by the embodiment of the present invention 1
The high rate performance curve graph of the material of preparation.
Specific embodiment
The specific embodiment of invention is described in detail with reference to the accompanying drawing, it is to be understood that protection model of the invention
It encloses and is not limited by the specific implementation.The test method of actual conditions is not specified in the following example, usually according to routine
Condition, or according to condition proposed by each manufacturer.
Embodiment 1
A kind of preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope provided in an embodiment of the present invention,
Specifically includes the following steps:
S1, the phenolic resin of 0.3g is added in the ethyl alcohol of 50ml, stirring and dissolving is subsequently added into the stannic oxide of 0.1g
Particle, ultrasonic reaction 4h, obtains reaction solution at 40 DEG C；
S2, the ammonium persulfate of 6.85g is added in the methanol-water solution (the volume ratio 1:1 of methanol and water) of 50ml, it is molten
Solution, obtains ammonium persulfate-methanol-water solution；
S3,2, the 5- dimercapto-1,3,4-thiadiazole of 1.5g is added in 50ml ethyl alcohol, mixed dissolution is then stirring
It mixes and reaction solution obtained in S1 is added under state, the cetyl trimethylammonium bromide of 0.5g is added, continues to stir, then dropwise
Ammonium persulfate-methanol-water solution obtained in S2 is added, for 24 hours, revolving obtains reactant for stirring；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, is then calcined at 800 DEG C under argon atmosphere
5h, cooled to room temperature to get arrive the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
Embodiment 2
A kind of preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope provided in an embodiment of the present invention,
Specifically includes the following steps:
S1, the phenolic resin of 0.5g is added in the ethyl alcohol of 80ml, stirring and dissolving is subsequently added into the titanium dioxide of 0.15g
Tin particles, ultrasonic reaction 4h, obtains reaction solution at 40 DEG C；
S2, the ammonium persulfate of 6.85g is added in the methanol-water solution (the volume ratio 1:1 of methanol and water) of 50ml, it is molten
Solution, obtains ammonium persulfate-methanol-water solution；
S3,2, the 5- dimercapto-1,3,4-thiadiazole of 1.5g is added in 50ml ethyl alcohol, mixed dissolution is then stirring
It mixes and reaction solution obtained in S1 is added under state, the cetyl trimethylammonium bromide of 0.5g is added, continues to stir, then dropwise
Ammonium persulfate-methanol-water solution obtained in S2 is added, for 24 hours, revolving obtains reactant for stirring；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, is then calcined at 900 DEG C under argon atmosphere
5h, cooled to room temperature to get arrive the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
Embodiment 3
A kind of preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope provided in an embodiment of the present invention,
Specifically includes the following steps:
S1, the phenolic resin of 0.4g is added in the ethyl alcohol of 50ml, stirring and dissolving is subsequently added into the stannic oxide of 0.2g
Particle, ultrasonic reaction 4h, obtains reaction solution at 40 DEG C；
S2, the ammonium persulfate of 7.85g is added in the methanol-water solution (the volume ratio 1:1 of methanol and water) of 50ml, it is molten
Solution, obtains ammonium persulfate-methanol-water solution；
S3,2, the 5- dimercapto-1,3,4-thiadiazole of 1.5g is added in 50ml ethyl alcohol, mixed dissolution is then stirring
It mixes and reaction solution obtained in S1 is added under state, the cetyl trimethylammonium bromide of 0.5g is added, continues to stir, then dropwise
Ammonium persulfate-methanol-water solution obtained in S2 is added, for 24 hours, revolving obtains reactant for stirring；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, is then calcined at 800 DEG C under argon atmosphere
5h, cooled to room temperature to get arrive the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
Embodiment 4
A kind of preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope provided in an embodiment of the present invention,
Specifically includes the following steps:
S1, the phenolic resin of 0.3g is added in the ethyl alcohol of 50ml, stirring and dissolving is subsequently added into the stannic oxide of 0.1g
Particle, ultrasonic reaction 4h, obtains reaction solution at 40 DEG C；
S2, the ammonium persulfate of 6.85g is added in the methanol-water solution (the volume ratio 1:1 of methanol and water) of 50ml, it is molten
Solution, obtains ammonium persulfate-methanol-water solution；
S3,2, the 5- dimercapto-1,3,4-thiadiazole of 3g is added in 50ml ethyl alcohol, mixed dissolution is then stirring
Reaction solution obtained in S1 is added under state, the cetyl trimethylammonium bromide of 1g is added, continues to stir, then be added dropwise
Ammonium persulfate-methanol-water solution obtained in S2, for 24 hours, revolving obtains reactant for stirring；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, is then calcined at 700 DEG C under argon atmosphere
5h, cooled to room temperature to get arrive the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
Comparative example 1
A kind of preparation method of porous carbon coating tin dioxide composite material, specific steps are same as Example 1, and difference is only
It is to be added without 2,5- dimercapto -1,3,4- thiadiazoles and ethyl alcohol in step S3.
Comparative example 2
Before the material of comparative example 2 is the porous uncoated carbon of carbon coating tin dioxide composite material that comparative example 1 provides
Stannic oxide particle.
We tie the porous carbon coating tin dioxide composite material of nitrogen sulphur codope of preparation by taking embodiment 1 as an example
Structure and Electrochemical Properties.
Fig. 1 is the specific surface of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope prepared by the embodiment of the present invention 1
Long-pending and graph of pore diameter distribution.From figure 1 it appears that the specific surface area of the composite material is 7.9308m2/ g, hole cumulative surface
Product is 10.6623m2/ g, accumulation pore volume are 0.040936cm3/ g, mainly mesoporous and micropore in composite material, illustrates to make
Standby composite material has porous structure, and aperture is about 1-30nm.
By the porous carbon coating tin dioxide composite material of nitrogen sulphur codope, carbon black, polyvinylidene fluoride according to 8:1:1 matter
Amount is matched and is ground after mixing with suitable N-Methyl pyrrolidone, electrode material is obtained, by electrode material coater
Coated on copper foil, in 80 DEG C of dry 3h, 12h is then dried in a vacuum drying oven, cell negative electrode material is obtained, in glove box
In using prepared negative electrode material as working electrode, lithium piece be to electrode, 1M LiPF6(ethylene carbonate, the carbon of 1:1 volume ratio
Dimethyl phthalate is mixed solvent) it is electrolyte, Celgard 2500 is diaphragm, is assembled into the button electricity of CR2025 model jointly
Pond.
Fig. 2 is prepared by the porous carbon coating tin dioxide composite material of nitrogen sulphur codope, comparative example 1 and 2 prepared by embodiment 1
Material 750 chemical property curve graphs are recycled under 100mA/g current density.From figure 2 it can be seen that embodiment 1
The porous carbon coating tin dioxide composite material cycle performance of nitrogen sulphur codope of preparation is substantially better than the cyclicity of comparative example 1 and 2
Can, there is excellent electrochemistry cycle performance, the porous carbon coating tin dioxide composite material of nitrogen sulphur codope prepared by embodiment 1
After recycling 750 times under 100mA/g current density, reversible capacity is still maintained at 854mAh/g.
Fig. 3 is prepared by the porous carbon coating tin dioxide composite material of nitrogen sulphur codope prepared by embodiment 1 and comparative example 1
The high rate performance curve graph of material, from figure 3, it can be seen that the porous carbon coating titanium dioxide of nitrogen sulphur codope prepared by embodiment 1
Tin composite material returns to 0.1Ag after recycling under 60 different current densities-1Current density after, capacity is almost
Do not decay.Compared to the material that comparative example 1 synthesizes, the porous carbon coating stannic oxide of nitrogen sulphur codope that embodiment 1 synthesizes is compound
Material has more superior specific discharge capacity and stability under time-dependent current.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, since the step method of use is identical as embodiment,
It repeats in order to prevent, the present invention describes preferred embodiment and its effect, and once a person skilled in the art knows bases
This creative concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (10)
1. a kind of preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope, which is characterized in that including following
Step:
S1, phenolic resin is added in organic solvent, stirring and dissolving is subsequently added into stannic oxide particle, reacts at 40 DEG C
4h obtains reaction solution, wherein the molar ratio of phenolic resin and stannic oxide particle is 2.5~4:1；
S2, ammonium persulfate is added in methanol-water solution, dissolves, obtains ammonium persulfate-methanol-water solution；
S3,2,5- dimercapto-1,3,4-thiadiazole is added in organic solvent, mixed dissolution, is then added under stirring
Enter reaction solution obtained in S1, cetyl trimethylammonium bromide is added, continues to stir, persulfuric acid obtained in S2 is then added
Ammonium-methanol-water solution, for 24 hours, revolving obtains reactant for stirring；Wherein, it is used in stannic oxide particle used in S1 and S2
Ammonium persulfate and mole with 2,5- dimercapto -1,3,4- thiadiazoles, cetyl trimethylammonium bromide used in S3
Than for 3~10:150~344:100:14；
S4, reactant obtained in S3 is reacted for 24 hours at 120 DEG C, then under protective gas atmosphere at 700~900 DEG C
Calcine 5h, cooled to room temperature to get arrive the porous carbon coating tin dioxide composite material of nitrogen sulphur codope.
2. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S1, the ratio of the phenolic resin and organic solvent is 0.3~0.5g:50ml.
3. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S2, the ratio of the ammonium persulfate and methanol-water solution is 6.85~7.85g:50ml.
4. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 3, special
Sign is, in step S2, the volume ratio of methanol and water is 1:1 in the methanol-water solution.
5. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S3, the ratio of 2, the 5- dimercapto-1,3,4-thiadiazole and organic solvent is 1.5~0.3g:50ml.
6. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S1 and S3, the organic solvent is acetone or dehydrated alcohol.
7. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S4, the protective gas is argon gas.
8. the preparation method of the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 1, special
Sign is, in step S4, the heating rate of the calcination process is 3 DEG C/min.
9. the porous carbon coating titanium dioxide of nitrogen sulphur codope that preparation method according to claim 1-8 is prepared
Tin composite material.
10. the porous carbon coating tin dioxide composite material of nitrogen sulphur codope according to claim 9 is on cathode of lithium battery
Application.
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